CN106517245B - A kind of method that ammonium chloride solution removes cobalt - Google Patents
A kind of method that ammonium chloride solution removes cobalt Download PDFInfo
- Publication number
- CN106517245B CN106517245B CN201611047017.8A CN201611047017A CN106517245B CN 106517245 B CN106517245 B CN 106517245B CN 201611047017 A CN201611047017 A CN 201611047017A CN 106517245 B CN106517245 B CN 106517245B
- Authority
- CN
- China
- Prior art keywords
- cobalt
- ammonium chloride
- solution
- chloride solution
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
- C05C3/005—Post-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention is a kind of ammonium chloride solution except cobalt method, in method, ammonium sulfide and super-fine cobalt powder is added in ammonium chloride solution, a small amount of cobalt ions in ammonium chloride solution precipitate in the form of cobalt sulfide, then Isolating chlorinated ammonium salt solution and cobalt sulfide precipitating.In the present invention, super-fine cobalt powder can be used as crystal seed, and induction cobalt sulfide is rapidly nucleated and grows on its surface, accelerate the precipitating of cobalt sulfide, and the microballoon of the cobalt sulfide cladding cobalt powder generated further plays catalytic action and reaction is accelerated to carry out, and reaction speed is accelerated.
Description
Technical field
The present invention relates to ammonium chloride solution purification and impurity removal technical fields, and particularly a kind of ammonium chloride solution removes the side of cobalt
Method.
Background technique
Ammonium chloride is a kind of important Nitrogenous fertilizer resources, is had a wide range of applications in agricultural production.Cobalt carbonate is to prepare electricity
The important source material of pond material cobaltosic oxide, carbonic acid cobalt precursor are to be prepared by cobalt chloride solution through ammonium bicarbonate precipitation
, reaction generates cobalt carbonate and ammonium chloride, and when filtering cobalt carbonate, ammonium chloride enters solution, and filtrate obtains after condensing crystallizing
Ammonia chloride crystal byproduct.But filter progress is precipitated in cobalt carbonate, have part cobalt ions Co2+Into solution, so that in chlorine
When changing ammonium salt solution condensing crystallizing, cobalt salt can be precipitated in ammonia chloride crystal simultaneously, and the ammonia chloride crystal crystallized out is caused to show secretly
Red, this not only seriously reduces the quality of ammonium chloride product, also results in the waste of expensive cobalt resource.
Summary of the invention
The above technical problem is not solved, a kind of method that the present invention devises new chemical precipitating is concentrated in ammonium chloride solution
Purification depth is carried out before crystallization to it and takes off cobalt processing, makes the Co in solution2+Removing.It is real that the present invention adopts the following technical solutions
Existing:
A kind of method that ammonium chloride solution removes cobalt, method include,
Ammonium hydroxide will be added in step 1 in ammonium chloride solution, adjust the pH value of solution to 7~8；
Step 2 is added ammonium sulfide and is stirred in adjusting the ammonium chloride solution after pH value, it reacts in solution, so
Super-fine cobalt powder is added in solution in backward reaction, obtains cobalt sulfide precipitating, then filters, precipitation and separation and filtrate；
Sodium hypochlorite powder is added in filtrate obtained in step 2 and heats and boils, until solution is clarified, obtains for step 3
To except the ammonium chloride solution after cobalt.
Preferably, in step 1, the concentration that ammonium hydroxide is added is 25%.
Preferably, in step 2, temperature when reacting in solution remains 35~40 DEG C.
Preferably, in step 2, the ammonium sulfide that is added in ammonium chloride solution to be excessive, excess coefficient is 1.15~
2.00, the amount that super-fine cobalt powder is added is the 1/3~1 of ammonium sulfide quality.
Preferably, in step 2, the partial size that super-fine cobalt powder is added is 6~10 μm.
It is highly preferred that after super-fine cobalt powder is added in the solution into reaction, continuing to keep 2~4h of reaction, so in step 2
It is filtered again afterwards.
Preferably, in step 3, temperature when reacting in solution remains 35~40 DEG C.
Preferably, it in step 3, heats and boils after addition sodium hypochlorite powder in filtrate, stir and maintain reaction in solution
20~40min.
In technical solution of the present invention, depth can be carried out to high strength ammonium-chloride solution and take off cobalt, so that in vaporizing raw liquor
Co2+Concentration drops to 0.2mg/L hereinafter, and can be to Co2+Concentration is recycled, and resource circulation utilization is promoted, and improves warp
Ji value.
In the present invention, ammonium sulfide is as precipitating reagent, due to ammonium sulfide and Co2+The cobalt sulfide precipitating particle that reaction generates is very
Carefully, it is easy to wear filter when filtering into solution, causes the pollution again of solution, super-fine cobalt powder is selected to can be used as crystal seed,
Induction cobalt sulfide is rapidly nucleated and grows on its surface, forms big vulcanization cobalt granule precipitating, and whole may be implemented in when filtering
Filtering, meanwhile, the cobalt sulfide precipitating of larger particles further functions as catalytic action, accelerates reaction and carries out.
In the solution of the present invention, experiment proves that, pH7~8 can reach optimal except cobalt effect, solution slant acidity (pH
< 6), ammonium sulfide is added and has hydrogen sulfide gas releasing；Meta-alkalescence pH > 8, OH in solution-And NH4 +It will form ammonium hydroxide, release ammonia
Gas, pH it is too high or too low all can degradation manipulation environment, therefore select pH for 7~8 optimization process programs.
Present invention process is simple, and raw material is suitable, and minimal amount of sulphur, the sodium ion introduced in reaction system is present in ammonium chloride
In crystal, fertilizer application can be used as, wherein minimal amount of sulphur and sodium ion do not influence the product quality of chemical fertilizer not only, also to plant
Many physiological functions of object go on smoothly very useful, therefore the present invention plays the effect of double gain.
Detailed description of the invention
Fig. 1 ammonium chloride solution of the present invention removes the method flow schematic diagram of cobalt
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
Ammonium chloride solution sample obtained in cobalt carbonate production is obtained, evaporation drying obtains the drying sample of ammonia chloride crystal,
And the 100g drying ammonia chloride crystal sample is taken, measuring the cobalt content in 100g ammonia chloride crystal is 0.0369%.
The 100g ammonia chloride crystal is dissolved completely in 400mL water and prepares solution, measures Co in the solution2+Concentration be
65.5mg/L, it is 8 that the pH value that ammonium hydroxide is adjusted in solution, which is added, and 0.1g ammonium sulfide is then added into solution, and adding D50 is 6 μ
The cobalt powder 0.05g of m, 35 DEG C of heating water bath, and stir, stop after 2h.Solution after reaction is filtered, washed, filter residue is collected and makees
For the raw material for mentioning cobalt, and 0.1g sodium hypochlorite powder is added into filtrate, continues heating and boil, be stirred to react 25min, solution becomes
For clarification, Co is not detected in filtering solution, filtrates tested ions content2+。
In this embodiment, a small amount of cobalt ions in ammonium chloride solution and ammonium sulfide, which react, generates cobalt sulfide, reacts
Ionic equation be Co2++(NH4)2S=CoS+2NH4 +.In the reaction, form removing of the cobalt sulfide of generation to precipitate, and
Excessive ammonium sulfide is introduced, therefore after addition sodium hypochlorite powder, the reaction occurred in solution is ClO-+S2-=SO4 2-+
4Cl-。
Embodiment 2
Ammonium chloride solution sample obtained in cobalt carbonate production is obtained, evaporation drying obtains the drying sample of ammonia chloride crystal,
And the 100g drying ammonia chloride crystal sample is obtained, measuring the cobalt content in 100g ammonia chloride crystal is 0.0369%.
The 100g ammonia chloride crystal is dissolved completely in 500mL water and prepares solution, measures Co in the solution2+Concentration be
52.4mg/L, it is 7.2 that the pH that ammonium hydroxide is adjusted in solution, which is added, and 0.08g ammonium sulfide is then added into solution, is D50 is added
10 μm of cobalt powder 0.05g 40 DEG C of heating water bath, is stirred, is reacted and stop after 2.5h.Solution after filtering reaction, collects filter respectively
Slag and filtrate obtain filtrate, and 0.11g sodium hypochlorite powder is added into filtrate, continue heating and boil, are stirred to react 40min, molten
Liquid becomes clarifying, filtering solution, and the ion concentration in filtrates tested, measures Co2+Content be 0.10mg/L.
Embodiment 3
Ammonium chloride stoste 1000mL obtained in cobalt carbonate production technology is taken, analysis obtains the Co in stoste2+Content is
53.6mg/L。
With mass fraction be 25% ammonium hydroxide adjust ammonium chloride solution pH be 8, be added ammonium sulfide 0.15g, be added D50 be 6 μm
Cobalt powder 0.1g, 40 DEG C of heating water bath, and stir, mixing speed 300r/min, react 2h.After reaction, reaction is molten
Liquid is filtered, washed, residue collection, about 0.12g sodium hypochlorite powder is added in collected filtrate, is continued heating and is boiled, stirs
It mixes under the conditions of speed is 300r/min and reacts 40min, solution becomes clear, colorless, filters to obtain ammonium chloride solution, filtrate inspection again
Measure Co2+Concentration be 0.18mg/L.
Embodiment 4
Ammonium chloride stoste 1000ml in cobalt carbonate production is taken, analysis obtains the Co in stoste2+Content 53.6mg/L.
With mass fraction be 25% ammonium hydroxide adjust ammonium chloride solution pH be 7.5, be added ammonium sulfide 0.15g, additions D50 be 9 μ
The cobalt powder 0.1g of m, 30 DEG C of heating water bath, and stir, mixing speed 300r/min, react 4h.After reaction, reaction is molten
Liquid is filtered, washed, residue collection, about 0.12g sodium hypochlorite powder is added in collected filtrate, is continued heating and is boiled, stirs
It mixes under the conditions of speed is 300r/min and reacts 35min, solution becomes clear, colorless, filters to obtain ammonium chloride solution, filtrate inspection again
Measure Co2+Concentration be 0.20mg/L.
Embodiment 5
Ammonium chloride stoste 1000ml in cobalt carbonate production is taken, analysis obtains the Co in stoste2+Content 53.6mg/L.
With mass fraction be 25% ammonium hydroxide adjust ammonium chloride solution pH be 8, be added ammonium sulfide 0.15g, be added D50 be 8 μm
Cobalt powder 0.1g, 40 DEG C of heating water bath, and stir, mixing speed 300r/min, react 3h.After reaction, reaction is molten
Liquid is filtered, washed, residue collection, about 0.12g sodium hypochlorite powder is added in collected filtrate, is continued heating and is boiled, stirs
It mixes under the conditions of speed is 300r/min and reacts 30min, solution becomes clear, colorless, filters to obtain ammonium chloride solution, filtrate inspection again
Measure Co2+Concentration be 0.20mg/L.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims
Subject to.
Claims (6)
1. a kind of method that ammonium chloride solution removes cobalt, which is characterized in that method includes,
Ammonium hydroxide will be added in step 1 in ammonium chloride solution, adjust the pH value of solution to 7~8；
Step 2 is added ammonium sulfide and is stirred in adjusting the ammonium chloride solution after pH value, reacted in solution, then to anti-
Super-fine cobalt powder is added in the solution answered, obtains cobalt sulfide precipitating, then filters, precipitation and separation and filtrate；The grain of super-fine cobalt powder
Diameter is 6~10 μm；
Sodium hypochlorite powder is added in filtrate obtained in step 2 and heats and boils, until solution is clarified, and mistake for step 3
Filter is obtained except the ammonium chloride solution after cobalt.
2. the method that a kind of ammonium chloride solution according to claim 1 removes cobalt, which is characterized in that in step 1, ammonia is added
The concentration of water is 25%.
3. the method that a kind of ammonium chloride solution according to claim 1 removes cobalt, which is characterized in that in step 2, in solution
Temperature when reaction remains 35~40 DEG C.
4. the method that a kind of ammonium chloride solution according to claim 1 or 3 removes cobalt, which is characterized in that in step 2, in chlorine
Change the ammonium sulfide being added in ammonium salt solution to be excessive, excess coefficient is 1.15~2.00, and the amount that super-fine cobalt powder is added is ammonium sulfide matter
The 1/3~1 of amount.
5. the method that a kind of ammonium chloride solution according to claim 4 removes cobalt, which is characterized in that in step 2, to reaction
In solution in be added super-fine cobalt powder after, continue keep reaction 2~4h, be then filtered again.
6. the method that a kind of ammonium chloride solution according to claim 1 removes cobalt, which is characterized in that in step 3, in filtrate
It heats and boils after addition sodium hypochlorite powder, stir and maintain and react 20~40min in solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611047017.8A CN106517245B (en) | 2016-11-23 | 2016-11-23 | A kind of method that ammonium chloride solution removes cobalt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611047017.8A CN106517245B (en) | 2016-11-23 | 2016-11-23 | A kind of method that ammonium chloride solution removes cobalt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106517245A CN106517245A (en) | 2017-03-22 |
| CN106517245B true CN106517245B (en) | 2019-02-19 |
Family
ID=58357956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611047017.8A Active CN106517245B (en) | 2016-11-23 | 2016-11-23 | A kind of method that ammonium chloride solution removes cobalt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517245B (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059241C (en) * | 1998-09-25 | 2000-12-06 | 孔令树 | Process for efficiently extracting cobalt compound from leftover containing cobalt |
| CN102432648B (en) * | 2010-09-29 | 2016-03-23 | 无锡济民可信山禾药业股份有限公司 | A kind of reactant takes off the method for cobalt and extraction |
| CN102492858A (en) * | 2011-12-22 | 2012-06-13 | 河南省冶金研究所有限责任公司 | Method for separating enriched nickel and cobalt from battery waste leaching solution |
| EP2882880B1 (en) * | 2012-08-09 | 2017-10-11 | Deepgreen Engineering Pte. Ltd. | Treatment of manganese-containing materials |
| FI125216B (en) * | 2013-05-23 | 2015-07-15 | Outotec Finland Oy | Method for recovering metals |
-
2016
- 2016-11-23 CN CN201611047017.8A patent/CN106517245B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106517245A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4316393B2 (en) | Calcium fluoride manufacturing method, recycling method and recycling method | |
| KR101093557B1 (en) | Method for treating phosphorus and nitrogen comprised in sewage or wastewater using iron ore wastewater | |
| CA2663108C (en) | Method of producing iron-arsenic compound excellent in crystallinity | |
| CN102432045B (en) | Preparation method of ultra-high purity lithium carbonate | |
| CA2845019A1 (en) | Treatment of phosphate-containing wastewater with fluorosilicate and phosphate recovery | |
| CN102612563B (en) | The preparation method of monovalence succinate | |
| JP2009285635A (en) | Phosphorus recovery material and method for recovering phosphorus | |
| CN109795995A (en) | A kind of method of hydrochloric acid method phosphoric acid by wet process efficient impurity removal | |
| CN102432046B (en) | Utilization method of chloride type salt lake brine | |
| CN105600763A (en) | Method for producing industrial monoammonium phosphate through fluoride salt purification method | |
| CN106517245B (en) | A kind of method that ammonium chloride solution removes cobalt | |
| CN107447256A (en) | A kind of method for preparing alkali formula magnesium iodide whisker | |
| CN110438347A (en) | Sodium cleans extraction vanadium method | |
| CN104556205B (en) | A kind of processing method utilizing the environmental protection of electrolytic zinc waste residue to produce feed level zinc sulfate | |
| CN109809377A (en) | A kind of method of sulfuric acid process phosphoric acid by wet process efficient impurity removal | |
| EA025514B1 (en) | Dihydrate-hemihydrate process for producing phosphoric acid | |
| CN111908499A (en) | Method and device for preparing copper oxide and ammonium chloride by combining waste acid and alkaline etching solution | |
| US9982315B2 (en) | Process including a carbonation step | |
| CN110512075A (en) | A kind of method of cobaltous sulfate manganese mixed liquor deeply purifying and removing cadmium | |
| CN106629776A (en) | Method for deeply removing cobalt ions in ammonium chloride solution | |
| JP2013245159A (en) | Method for comprehensively treating claus tail gas and producing manganese sulfate | |
| CN103288133A (en) | Method for preparing arsenic trioxide from black copper sludge | |
| CN106800303A (en) | A kind of method that utilization micro passage reaction prepares KI | |
| CN102086026A (en) | Method for producing potassium chlorate and co-producing superfine calcium carbonate and ammonium chloride by utilizing carbide slag | |
| CN111484039A (en) | Method for removing sodium/potassium carbonate and sodium/potassium hydroxide in sodium cyanide/potassium solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |